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United States Patent Office Patented Nov 2,860,951 United States Patent Office Patented Nov. 18, 1958 ee. sa has proven to be technologically or economically unat tractive. My invention comprises a combination of the first an 2,860,951 last of these approaches. Polyhalite deposits are found RECOVERY OF WALUES IN NATURALLY OCCUR 5 at depths ranging from 700 to 2000 feet and are often RNG ALKAL METAL SULFATE MENERALS interspersed with intrusions of halite (NaCl) and anhydrite George L. Cuzaningham, Cleveland Heights, Ohio, as (CaSO4). Polyhalite as mined in many instances con signor to Horizons incorporated tains as much as 13% sodium chloride, the removal of which is generally effected prior to any other treatment No Drawing. Application July 28, 1955 O of the ore in order to improve the recovery of potassium Seria No. 525,084 salts in the subsequent steps. The process variables to be considered in removal of the sodium chloride are dis 10 Claims. (CI. 23-32) cussed in detail in the aforesaid Bureau of Mines Bulletin. i have found that by rapid washing of the ore with This invention relates to a new and novel process for limited amounts of water at room temperature, over 95% the recovery of the alkali metal values in artificial or of the sodium chloride may be removed with an accom naturally occurring complex sulfates of alkali metals and panying loss of less than about 3% of the potassium sul one or more other metals, including calcium, magnesium, fate. Leaching with water at higher temperatures on the copper, manganese, lead, and aluminum. More particu order of 100° C. has been found to be unsuitable because larly it relates to a process in which the sulfate containing of the large amount of potassium sulfate lost in the ex material is sintered or fused with a proportioned amount traction liquid. of acid oxide such as silica sand under conditions which After the sodium chloride has been removed by rapid insure the conversion of the other metal content of the washing, the polyhalite is heated with an acidic oxide, charge material from the sulfate to the silicate without preferably silica (SiO2) to a temperature between about any appreciable accompanying conversion of the alkali 500° C. and 1500° C. or even higher. As a result, the metal sulfate content of the charge material. alkaline earth Suifates are converted to alkaline earth Typical minerals which are amenable to the process silicates and sulfur dioxide is evolved from the heated constituting my invention include the following natural 2SS. - - - - - - - - - - or artificial ores: By varying the ratio of silica to polyhalite used in the 30 sintering or fusion operation, more or less of the alkaline earth content of the polyhalite is converted to the corre Name Formula sponding silicate. It is preferred to use an amount of Palmierite----------------------- (K,Na)2SO4.PbSO4 silica which is exactly stoichiometrically equal to the Vanthoffite----- 3Na2SO4.MgSO4 amount required to react with the alkaline earth sulfates, Glauberite--- -- Na2SO4.CaSO4 35 Langbeinite----- - K2SO4.2MgSO4 i. e. the calcium sulfate and magnesium sulfate, in the Manganolangbeinite K2SO4.2MnSO Syngenite.-- K2SO4·CaSO4.H2O polyhalite. When the amount of silica used is in excess Kroehnkite- Na2SO4.CuSO4.2H2O of the stoichiometric amount required to react with the Toewite--- Na2SO4.MgSO4.2%H2O Bloedite--------- - Na2SO4.MgSO4.4H2O calcium sulfate and magnesium sulfate in the polyhalite, Wattevilleite--- n Na2SO4. CaSO4.4H2O then small amounts of potassium silicate may be formed Leonite---------- K2SO4.MgSO4.4H2O 40 by reaction with the excess. When the amount of silica Picromerite- K2SO4.MSO4.6H2O used is less than the amount required to react with both CyanochroitePolyhalite- K2SO4.2CaSO4.MgSO4.2H2OK2SO4.CuSO4.6H2O Leightonite- K2SO4.2CaSO4.CuSO4.2H2O the calcium sulfate and the magnesium sulfate, it has been Tamarugite- -- Na2SO4. Al2(SO4)3.12129 found that the silica preferentially reacts with the mag Mendozite---- - Na2SO4·Al2(SO4)3.22H2O Kalinite ---------- - K2SO4·Al2(SO4)3.22H2O nesium sulfate, leaving some or all of the calcium sulfate Potassium Alum--- in the polyhalite unreacted. Sodium Alum. Aiunite----- K2SO4.3Al2(SO4)3(OH)4 In order to obtain rapid reaction between the silica and Natroakunite Na2SO4.3Al2(SO4)3(OH)4 the polyhalite, I have found it advantageous to grind the Natrochalcit Na2SO4.3CuSO4.Cu(OH)2.2O sand and polyhalite prior to mixing the two ingredients. The reactants need not be dried since the presence of and others of even greater complexity. Because there are 50 small announts of water vapor has been found to be bene extensive deposits of polyhalite in the United States and ficial in the conversion of Stilfate to silicate. other parts of the world, and because the procedures are The silica used in the process need not be of high purity typical, this specification will describe the treatment of and ordinary sand as been found to be very suitable. polyhalite, it being usaderstood that tie techniques dis However, if the calcium silicate and magnesium silicate closed are equally applicable to the processing of many 55 are to be sold as white pigments or fillers, the sand used other naturally occurring ores or artificially groduced sui should be relatively low in iron and other impurities. fate containing minerals, such as hose listed above. Whatever the ratio of silica to polyhalite, the product Numerous efforts have been made to devise and to de of the sintering or fusion operation is next preferably velop processes for the recovery of potassium sulfate and leached with hot water. By extracting the residue from other salts from polyhalite, but until the present time the sintering operation with limited amounts of hot water no method has been successfully commercially exploited. it is possible to obtain solutions which are substantially The Bureau of Mines of the United States Department saturated with respect to potassium sulfate. Depending of the Interior has carried out extensive investigations on the recovery of various potassium salts from polyhalite on the ratio of silica to polyhalite, the extracts may also and has published a comprehensive report on the subject. contain unreacted alkaline earth sulfates or small amounts in Bulletin 459. Three general lines of investigation are of potassium silicate when excess silica is employed. discussed in the report as follows: (1) solution processes Although the potassium sulfate in the sintered mass employing no added chemicals other than water and pos has been found to be readily soluble in hot or cold water, sibly heat (2) reduction of the sulfates to sulfides or I have found that the extraction may be effected with oxides prior to solution processes and (3) decomposition minimal amounts of water by crushing the sintered prod by chemical reaction with various reagents such as lime, uct, or by quenching the fusion product directly in water carbon dioxide or ammonia. Each of these lines of attack and wet grinding the frit so produced. By extracting the 2,860,951 3 4 solid, crushed, ground or fritted residue with water at with respect to potassium sulphate which was recovered, 100 C. in counter current fashion, I have produced as previously described, by cooling the solution and per aqueous solutions containing approximately 24.1 grams mitting the potassium sulfate to crystalline out. The of potassium sulfate per 100 grams of water. On cool crystals were recovered by filtration, washed clean of ing the extract to 25 C., about one half of the potassium 5 mother liquor and then dried. The solid residue remain sulfate is precipitated as a crystalline product which is ing after repeated extractions with hot water was almost easily removed by filtration. The filtrate, or mother entirely pure calcium silicate, which when dried in use liquor, is reheated to 100° C. and employed to extract ful as a pigment, filler or soil conditioner. more potassium sulfate from the solid residue produced during the sintering or fusion step. The material remain O Example 3 ing after repeated washings is composed almost entirely The process of Example 2 was repeated except that of calcium silicate and magnesium silicate. Fresh water hot water was used to extract the magnesium sulfate from is employed to remove the last traces of potassium or the calcined polyhalite. The solid phase remaining was other soluble salts, the wash water being returned to potassium calcium pentasulfate (K2SO4.5CaSO4·H2O) the counter current extraction stage. The washed solid 5 instead of a mixture of syngenite and gypsum. The silicates are heated to remove water and when free of potassium calcium pentasulfate was . crushed and then moisture form a white powdered solid suitable as an intimately mixed with sufficient silica to convert the inert filler, or as a pigment, or as a corrective addition calcium sulfate to calcium silicate. The mixture was to acid soils. The following example of the process is sintered at about 900° C. for 30 minutes, after which the given by way of illustration and is not to be taken as 20 potassium sulfate was extracted with hot water. The limitative thereof. residue, calcium silicate, was dried and recovered as a Example I fine white, pigment grade powder. The potassium sul A mixture was formed comprising 22 parts by weight fate crystallized out of the extraction liquor when it was of silica which has been ground to -200 mesh (Tyler cooled to room temperature and was separated therefrom. Standard) and 65 parts of finely divided, -325 mesh 25 Example 4 (Tyler Standard) polyhalite. The polyhalite analyzed In still another variation of my process, polyhalite was 12.65% potassium, by weight; 4.8% magnesium, by rapidly leached free of halite and then calcined. The weight; 11.58% calcium, by weight; 60.96% sulfate, by calcine was extracted with a saturated solution of potas weight; and 2.92% sodium chloride.
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